US8273927B2 - Alcohol fractionation - Google Patents
Alcohol fractionation Download PDFInfo
- Publication number
- US8273927B2 US8273927B2 US12/858,566 US85856610A US8273927B2 US 8273927 B2 US8273927 B2 US 8273927B2 US 85856610 A US85856610 A US 85856610A US 8273927 B2 US8273927 B2 US 8273927B2
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- US
- United States
- Prior art keywords
- alcohol
- solution
- caustic
- aqueous
- phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related, expires
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000005194 fractionation Methods 0.000 title description 4
- 239000000243 solution Substances 0.000 claims abstract description 16
- 239000003518 caustics Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 238000011084 recovery Methods 0.000 claims abstract description 3
- 238000004064 recycling Methods 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008346 aqueous phase Substances 0.000 claims description 4
- 238000010924 continuous production Methods 0.000 claims description 2
- 238000005192 partition Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 3
- 230000008020 evaporation Effects 0.000 claims 3
- 238000000034 method Methods 0.000 abstract description 17
- 238000005191 phase separation Methods 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 238000004821 distillation Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 235000013522 vodka Nutrition 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000002864 food coloring agent Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- KVMUSGMZFRRCAS-UHFFFAOYSA-N sodium;5-oxo-1-(4-sulfophenyl)-4-[(4-sulfophenyl)diazenyl]-4h-pyrazole-3-carboxylic acid Chemical compound [Na+].OC(=O)C1=NN(C=2C=CC(=CC=2)S(O)(=O)=O)C(=O)C1N=NC1=CC=C(S(O)(=O)=O)C=C1 KVMUSGMZFRRCAS-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000012756 tartrazine Nutrition 0.000 description 1
- 239000004149 tartrazine Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/94—Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
Definitions
- This invention relates to a process for the partition of an aqueous alcohol solution into two fractions, an alcohol phase and a water phase.
- an alkali metal hydroxide is added to the aqueous alcohol solution, thus causing the solution to undergo a phase separation.
- the resulting phases are evaporated to recover the alkali metal hydroxide, which is recycled in the process.
- distillation While effective in this application, distillation has several drawbacks.
- a primary disadvantage of distillation is that it consumes considerable amounts of energy. Thus, as much as 50 to 80 percent of the energy required to produce ethanol in a typical fermentation process is consumed in the distillation step.
- An added problem in producing absolute alcohol is that an azeotrope or constant boiling solution is formed during distillation.
- Ethanol for example, produces an azeotropic composition of 95 weight percent alcohol and the balance water.
- Isopropyl alcohol has a binary azeotrope of 91 weight percent alcohol, the rest being water.
- a process for the fractionation of alcohol from aqueous solutions of alcohol.
- caustic comprising an alkali metal hydroxide is added to the solution to produce a phase separation.
- water is separated from the alcohol.
- the resulting two streams are evaporated in order to recover the caustic, which can be recycled to the addition step.
- the alkali metal hydroxide includes the hydroxides of any alkali metal.
- sodium hydroxide as well as potassium hydroxide are eminently suitable.
- the solubilities of these hydroxides govern the level of their addition.
- the process of the present invention has general applicability. For example, it can be used to produce ethanol of any concentration. It can also be applied to the manufacture of isopropyl alcohol. Additionally, the process is applicable to butyl alcohol synthesis.
- FIG. 1 is a block diagram showing the principal steps of the process, including the addition of hydroxide to the alcohol solution and the recovery of the hydroxide.
- the process of the present invention can be conducted either as a batch operation or as a continuous process.
- an alkali metal hydroxide is added to a tank 1 containing an aqueous alcohol solution.
- aqueous alcohol solution for example, flaked sodium hydroxide can be introduced in to a tank of 20% ethanol. Alternatively 73% caustic soda can be used.
- Mixing is provided by any effective means of agitation. Cooling coils or tank jacketing are preferably used to remove the heat of solution. Given the corrosive nature of caustic, the equipment is best fabricated from suitable alloys.
- Each of the streams from the mixing tank is sent to a separate evaporator 2 or 3 to remove the dissolved caustic. In this manner, an alcohol product is obtained while a waste aqueous stream is produced. Depending on product specifications, additional treatment may be required to manufacture the finished product.
- the evaporators 2 , 3 used are of standard design. Energy efficiency and investment cost are of prime consideration.
- mixing tank 1 receives the alcohol solution and caustic additive.
- Evaporator 2 separates the alcohol product from the dissolved caustic. By recycling the caustic streams, a self-contained process is achieved.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A process is provided for the recovery of alcohol from its aqueous solution by dissolving caustic in the solution to generate a phase separation. One layer contains the alcohol product and the other layer waste water. By recovering and recycling the caustic, a self-contained process is realized.
Description
This invention relates to a process for the partition of an aqueous alcohol solution into two fractions, an alcohol phase and a water phase. In the process, an alkali metal hydroxide is added to the aqueous alcohol solution, thus causing the solution to undergo a phase separation. The resulting phases are evaporated to recover the alkali metal hydroxide, which is recycled in the process.
Many processes for the manufacture of alcohols produce an intermediate stream comprising an aqueous alcohol solution. This solution must be fractionated in order to produce the final alcohol product.
The accepted practice for the fractionation of alcohol solutions is to use distillation. While effective in this application, distillation has several drawbacks. A primary disadvantage of distillation is that it consumes considerable amounts of energy. Thus, as much as 50 to 80 percent of the energy required to produce ethanol in a typical fermentation process is consumed in the distillation step.
An added problem in producing absolute alcohol is that an azeotrope or constant boiling solution is formed during distillation. Ethanol, for example, produces an azeotropic composition of 95 weight percent alcohol and the balance water. Isopropyl alcohol has a binary azeotrope of 91 weight percent alcohol, the rest being water.
To circumvent the limitations posed by azeotropes, several creative procedures have been used. The classic method of producing anhydrous ethanol is to use benzene to break the azeotrope. This approach, however, introduces a toxic impurity. A newer technique is to resort to the use of molecular sieves to dehydrate the alcohol.
It is an object of the present invention to provide a process for the fractionation of alcohol that is energy efficient, easy to apply, and adaptable to the production of large quantities of alcohol. This and other objects, features and advantages of the present invention will become apparent from the following description and the FIGURE that is included.
A process is provided for the fractionation of alcohol from aqueous solutions of alcohol. In the process, caustic comprising an alkali metal hydroxide is added to the solution to produce a phase separation. In this manner, water is separated from the alcohol. The resulting two streams are evaporated in order to recover the caustic, which can be recycled to the addition step.
The alkali metal hydroxide includes the hydroxides of any alkali metal. Thus, sodium hydroxide as well as potassium hydroxide are eminently suitable. The solubilities of these hydroxides govern the level of their addition.
The process of the present invention has general applicability. For example, it can be used to produce ethanol of any concentration. It can also be applied to the manufacture of isopropyl alcohol. Additionally, the process is applicable to butyl alcohol synthesis.
Other applications of the present invention will become apparent to those skilled in the art when the following description of the best mode contemplated for practicing the invention is read in conjunction with the accompanying drawings.
The description herein makes reference to the accompanying drawings wherein like reference numerals refer to like parts throughout the several views and wherein:
The process of the present invention can be conducted either as a batch operation or as a continuous process. In the batch mode of operation, an alkali metal hydroxide is added to a tank 1 containing an aqueous alcohol solution. For example, flaked sodium hydroxide can be introduced in to a tank of 20% ethanol. Alternatively 73% caustic soda can be used. Mixing is provided by any effective means of agitation. Cooling coils or tank jacketing are preferably used to remove the heat of solution. Given the corrosive nature of caustic, the equipment is best fabricated from suitable alloys.
Upon addition of the alkali metal hydroxide, a phase separation occurs almost immediately. The top layer contains alcohol and the bottom layer water. The alcohol phase is decanted while the aqueous phase is drained from the bottom of the tank. Even though the interface is clearly defined, careful control over the separation should be followed.
Each of the streams from the mixing tank is sent to a separate evaporator 2 or 3 to remove the dissolved caustic. In this manner, an alcohol product is obtained while a waste aqueous stream is produced. Depending on product specifications, additional treatment may be required to manufacture the finished product. The evaporators 2, 3 used are of standard design. Energy efficiency and investment cost are of prime consideration.
The present invention can better be visualized by referring to the schematic flow sheet of FIG. 1 . In this diagram, mixing tank 1 receives the alcohol solution and caustic additive. Evaporator 2 separates the alcohol product from the dissolved caustic. By recycling the caustic streams, a self-contained process is achieved.
- 1. In this experiment, 40.3 gm. of sodium hydroxide ACS crystals was dissolved in 200 ml. 80 proof vodka containing 40% ethyl alcohol by volume. Three drops of green food color containing FD&C Yellow 5 and FD&C Blue 1 was added. The warm solution separated into two phases; a top layer brightly colored red and a bottom layer that was clear yellow. The total volume of both phases was 204 ml. and the interface was at 96 ml. When a sample of the top layer was lit, it burned vigorously.
- 2. Similarly to example 1, 71.1 gm. of sodium hydroxide was dissolved in 100 ml. water and 100 ml. 80 proof vodka. A phase separation occurred, the aqueous phase equaling 180 ml. and the alcohol phase having a volume of 29 ml.
- 3. Instead of ethanol, isopropyl alcohol was used in this run. A total of 56.8 gm. of sodium hydroxide was added to approximately 200 ml. of 70% rubbing alcohol comprising isopropyl alcohol and water. Not all of the caustic was dissolved, but a phase separation immediately formed. The top layer of alcohol equaled 146 ml. and the bottom aqueous layer totaled 64 ml.
- 4. Finally, 155.2 gm. of potassium hydroxide was dissolved in 200 ml. of 80 proof vodka. A distinct phase separation was observed. The total volume of both phases was close to 262 ml. and the interface was at 165 ml.
Claims (1)
1. A continuous process for the recovery of alcohol from an aqueous solution of the alcohol comprising the steps of:
adding caustic to the solution to cause the partition of the solution into an alcohol rich phase and an aqueous phase;
separating the two phases;
recovering alcohol from the alcohol rich phase by evaporation;
removing water from the aqueous phase by evaporation; and
recycling streams of dissolved caustic from each of the evaporation steps to the addition step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12/858,566 US8273927B2 (en) | 2010-08-18 | 2010-08-18 | Alcohol fractionation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12/858,566 US8273927B2 (en) | 2010-08-18 | 2010-08-18 | Alcohol fractionation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| US20120046504A1 US20120046504A1 (en) | 2012-02-23 |
| US8273927B2 true US8273927B2 (en) | 2012-09-25 |
Family
ID=45594596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US12/858,566 Expired - Fee Related US8273927B2 (en) | 2010-08-18 | 2010-08-18 | Alcohol fractionation |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US8273927B2 (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1452206A (en) * | 1920-03-08 | 1923-04-17 | Seth B Hunt | Means for dehydrating alcoholic liquids |
| US2668863A (en) * | 1952-01-11 | 1954-02-09 | Standard Oil Dev Co | Purification of alcohols |
| US2949427A (en) * | 1957-10-17 | 1960-08-16 | Monsanto Chemicals | Breaking of oxo alcohol emulsions |
| US3689371A (en) * | 1967-12-20 | 1972-09-05 | Horst Kerber | Recovery of butanols plural stage distillation and alkali metal hydroxide treatment |
| US4454359A (en) * | 1982-06-21 | 1984-06-12 | The Procter & Gamble Company | Process for drying alcohols |
| US4594466A (en) * | 1984-08-22 | 1986-06-10 | Apace Research Limited | Recovery of alcohols |
| US4743707A (en) * | 1985-01-22 | 1988-05-10 | Showa Denko Kabushiki Kaisha | Process for purifying allyl alcohol |
-
2010
- 2010-08-18 US US12/858,566 patent/US8273927B2/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1452206A (en) * | 1920-03-08 | 1923-04-17 | Seth B Hunt | Means for dehydrating alcoholic liquids |
| US2668863A (en) * | 1952-01-11 | 1954-02-09 | Standard Oil Dev Co | Purification of alcohols |
| US2949427A (en) * | 1957-10-17 | 1960-08-16 | Monsanto Chemicals | Breaking of oxo alcohol emulsions |
| US3689371A (en) * | 1967-12-20 | 1972-09-05 | Horst Kerber | Recovery of butanols plural stage distillation and alkali metal hydroxide treatment |
| US4454359A (en) * | 1982-06-21 | 1984-06-12 | The Procter & Gamble Company | Process for drying alcohols |
| US4594466A (en) * | 1984-08-22 | 1986-06-10 | Apace Research Limited | Recovery of alcohols |
| US4743707A (en) * | 1985-01-22 | 1988-05-10 | Showa Denko Kabushiki Kaisha | Process for purifying allyl alcohol |
Also Published As
| Publication number | Publication date |
|---|---|
| US20120046504A1 (en) | 2012-02-23 |
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